CN101168625B - Intelligent temperature-control functional mica vanadium nacreous pigment and preparation thereof - Google Patents
Intelligent temperature-control functional mica vanadium nacreous pigment and preparation thereof Download PDFInfo
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- CN101168625B CN101168625B CN2007100506386A CN200710050638A CN101168625B CN 101168625 B CN101168625 B CN 101168625B CN 2007100506386 A CN2007100506386 A CN 2007100506386A CN 200710050638 A CN200710050638 A CN 200710050638A CN 101168625 B CN101168625 B CN 101168625B
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- 239000010445 mica Substances 0.000 title claims abstract description 55
- 229910052618 mica group Inorganic materials 0.000 title claims abstract description 55
- 239000000049 pigment Substances 0.000 title claims abstract description 50
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 23
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 49
- 230000007704 transition Effects 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000000137 annealing Methods 0.000 claims description 15
- 230000008859 change Effects 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 239000003595 mist Substances 0.000 claims description 3
- 230000002829 reductive effect Effects 0.000 claims description 3
- 238000005275 alloying Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000005457 optimization Methods 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims 5
- 229910052721 tungsten Inorganic materials 0.000 claims 5
- 238000001035 drying Methods 0.000 claims 1
- 238000005530 etching Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 claims 1
- 239000000155 melt Substances 0.000 claims 1
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000004381 surface treatment Methods 0.000 claims 1
- 238000009736 wetting Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000002932 luster Substances 0.000 abstract description 3
- 230000005855 radiation Effects 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 238000009413 insulation Methods 0.000 abstract 2
- 229910052751 metal Inorganic materials 0.000 abstract 2
- 239000002184 metal Substances 0.000 abstract 2
- 238000002834 transmittance Methods 0.000 abstract 2
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 abstract 1
- 238000005034 decoration Methods 0.000 abstract 1
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 229910001935 vanadium oxide Inorganic materials 0.000 abstract 1
- 239000010408 film Substances 0.000 description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- 239000011259 mixed solution Substances 0.000 description 12
- 150000002978 peroxides Chemical class 0.000 description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 description 6
- 239000004417 polycarbonate Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000003252 repetitive effect Effects 0.000 description 6
- 238000005201 scrubbing Methods 0.000 description 6
- 230000009466 transformation Effects 0.000 description 6
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 5
- 230000032683 aging Effects 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 108010025899 gelatin film Proteins 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
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- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention relates to mica vanadium pearly pigment which can realize the intelligent temperature control function. The pigment is compounded by flake-shaped mica powder and oxide film V1-xMxO2 of vanadium deposited on the surface of the flake-shaped mica powder. The V1-xMxO2 film has typical semiconductor-metal phase transition, when the temperature is higher than the phase transition temperature, the V1-xMxO2 is in a metal state, the infrared light transmittance is low, and the heat radiation of the infrared light can be decreased to play the heat insulation function; when the temperature is lower than the phase transition temperature of the film, the V1-xMxO2 is in a semiconductor state, the infrared light transmittance is high, and the ambient infrared ray can be fully utilized to realize the thermal insulation effect. The mica vanadium pearly pigment maintains the special color and the luster of the traditional pearly pigment, and the decoration effect is good; because vanadium oxide film takes the flake-shaped mica powder as a carrier, the parallel distribution of the flake-shaped mica in the medium can improve the intelligent temperature control efficiency of the pigment, and save the pigment cost. The invention has the advantages that the industrial preparation is simple, the cost is inexpensive, the product application is widespread, and the implementation of the invention can play the functions of saving the energy and protecting the environment.
Description
Technical field
The present invention relates to a kind of intelligent temperature-control functional mica vanadium nacreous pigment and preparation method thereof; The variation that this functional pigment has according to envrionment temperature changes the ability that sees through or shield sunshine mid-infrared light line, thereby realizes the intelligent control to its covering space temperature.Be particularly related to a kind of V
1-xM
xO
2/ mica intelligent temperature-control functional pearly pigment, pigment is by the sheet mica micro mist and cover its surperficial V
1-xM
xO
2Film be composited (film optimize thickness 30-300nm).It belongs to the functional inorganic material preparation field.
Background technology
Nineteen fifty-nine F.J.Morin has found VO first
2The thermal induced phase transition characteristic, monocrystalline VO
2At 68 ℃ the significantly first-order phase transition from the monoclinic form semi-conductor to cubic rutile crystal type metallographic phase can take place, follow phase transition process that crystalline specific refractory power, electric conductivity, susceptibility and infrared transmission, reflectivity sudden change can take place.Utilize these performances, VO
2Powder and thin-film material can be applied in fields such as room temps control, sensing, optical storage, light-operated, lasing safety.VO
2Material is when phase transformation, and infrared transmittivity can be undergone mutation, and when being higher than transformation temperature, has lower infrared transmittivity, has higher infrared transmittivity when being lower than transformation temperature.Ir radiation is the principal mode of energy emission in the sunshine, and the near infrared light energy accounts for 50% of sunshine total energy, at present about VO
2Powder body material or VO
2The applied research of thin-film material aspect intelligent temperature control mainly concentrates on micron order or nano level VO
2In the preparation and the application in products such as glass, plastics film thereof of powder.(J.Phy.Chem.Solids 2001,62:1229-1238) studied VO for F.Guinneton etc.
2Film and VO
2Particle is in the optical property of infrared light region.The result shows, successive VO
2Film is than the VO that is dispersed in the medium
2Micro-nano powder pigment has bigger infrared transmittivity before and after phase transformation changes and more high efficiency optical switch effect.But since preparation technology's restriction, big area VO
2The preparation difficulty of film is big, and cost is high.It is carrier that the present invention adopts flaky mica powder, coats one deck V on its surface
1-xM
xO
2Film.The mica sheet of high thickness to diameter ratio in applicating medium, have can parallel distribution characteristic, can form the successive resist, so with traditional spherical VO
2Pigment is compared, flaky V
1-xM
xO
2/ pigments, mica can improve under the coating high-temp reflectivity to infrared light; Can produce better intelligent temperature control effect when being applied in this sheet functional pigment in the products such as paint, glass, plastics film, as be applied to just can to reduce in car paint and the glass temperature and the room temp of sunlight in summer in getting off.
Prepare VO at present
2The technology of film or powder is more, and be mainly reflected in and sol-gel method prepares the advantage of functional mica vanadium nacreous pigment: preparation technology is simple relatively, and is not high to equipment requirements; Be fit to scale operation, material and the shape need to body material is not high simultaneously, is easier to be implemented in the thin film deposition on the various lopsided base materials; Realize easily mixing and preparation multicomponent metal oxide film.This method can effectively improve V
1-xM
xO
2The application performance of/nacreous mica pigment, and be V
1-xM
xO
2The suitability for industrialized production and the application of/nacreous mica pigment provide feasibility.
Summary of the invention
The purpose of this invention is to provide a kind of intelligent temperature-control functional mica vanadium nacreous pigment and preparation method thereof, adopt sol-gel and annealing reductive method at sheet mica micro mist surface deposition one deck V
1-xM
xO
2Film forms, and the optimization thickness of film is 30-300nm.When temperature is lower than V
1-xM
xO
2During the thin film phase change temperature, the infrared transmittivity of pigment is higher, when temperature is higher than transformation temperature, and V
1-xM
xO
2The infrared transmittivity of film reduces, and the thermal radiation of the variation control infrared light through envrionment temperature realizes intelligent temperature control.Pigment provided by the invention has kept the unique color and luster effect of traditional pearly pigment, has given the functional of pigment intelligent temperature control simultaneously.Can prepare mica vanadium nacreous pigment through method provided by the invention, satisfy the different demands of domestic and international market with different pearly-lustre colors and intelligent temperature control function.
Intelligent temperature-control functional mica vanadium nacreous pigment provided by the invention is to realize through following technological method:
1, with highly purified V
2O
5Powder 2.0～5.0 grams are heated in retort furnace more than 550, are molten state, pour into rapidly then in the deionized water, stir 2～5 hours after-filtration and promptly form V
2O
5Colloidal sol.When to VO
2When film mixes, at pure V
2O
5Add the compound that contains alloying element in the powder,
Doping ratio 0-0.25As: when mixing Mo, can add molybdenum acid ammonia; When mixing W, can add Tungsten oxide 99.999.
2, get an amount of mica powder successively at absolute ethyl alcohol, the mixed solution of hydrochloric acid and ydrogen peroxide 50 (volume ratio 2: 5) boiled respectively 0.5～2 hour in the mixed solution of ammoniacal liquor and ydrogen peroxide 50 (volume ratio 2: 5).With behind the deionized water repetitive scrubbing 100 ℃ of oven dry;
3, mica powder and vanadium colloidal sol are mixed according to a certain percentage, moisture evaporate to dryness is wherein incited somebody to action in heating in the time of stirring, and dried gel promptly is coated on the surface of mica powder, and different coating number of times can change the gel film thickness on the mica powder surface.
4, place tube furnace to be heated to 400 ℃～650 ℃ gained powder in the step 3, annealing reduction 0.5～6 hour.Be chosen under inert atmosphere or the reducing atmosphere and carry out, like Ar, N
2, H
2, gas flow rate: 5～60ml/min.
Compare with existing intelligent temperature-control functional pigment, the present invention has following advantage:
1. pigment utilizes the micaceous sheet structure, can improve that pigment has improved the intelligent temperature control performance of pigment to the shield effectiveness of infrared light when being higher than transformation temperature;
2. giving functional while of pigment has also kept the special color and luster effect of pearly pigment;
3. because V
1-xM
xO
2Content ratio in intelligent temperature-control functional mica vanadium nacreous pigment is not high, with respect to traditional intelligent temperature control functional pigment (pure V
1-xM
xO
2Powder), reduced the pigment cost.
4. the raw material that adopts is simple, only needs flaky mica powder and high-purity V
2O
5
5. technology is simple, less demanding to equipment;
Description of drawings
Fig. 1 is the V that has added the present invention's preparation
1-xM
xO
2The infrared permeation spectrum of the polycarbonate of/mica functional pigment (PC) film (pigment content is 1%) testing film under differing temps.Its result shows, at 2000cm
-1～4000cm
-1The infrared transmittivity of 100 ℃ of following films will be lower than the transmitance of film about 30% under the normal temperature in the scope.(explain: because the stretching vibration and the flexural vibration of c h bond in the PC resin make it at 2800cm
-1～3050cm
-1There is stronger absorption in wave band to infrared light, causes having added among the figure V
1-xM
xO
2The PC film of/mica functional pigment changes under 100 ℃ of high temperature and normal temperature not quite in the transmitance of this wave band.)
Fig. 2 is the V that has added the present invention's preparation
1-xM
xO
2The infrared light transmitance of the PC film of/mica functional pigment (the infrared light wavelength is 4 microns) is with the variation tendency of temperature change, and presentation of results adds the V of the present invention's preparation
1-xM
xO
2Sudden change has taken place in the infrared transmittivity of/micaceous PC film near 68 ℃, and change procedure is reversible.
Embodiment
Below through embodiment the present invention is further explained:
Embodiment 1
1. with 5.0gV
2O
5Powder is poured melt in the 400ml deionized water into 800 ℃ of following heat fused 30 minutes then, stirs fast 2 hours, obtains dark-brown V after the filtration
2O
5Colloidal sol was with still aging 48 hours of colloidal sol;
2. get the 5.0g white mica powder successively at absolute ethyl alcohol, the mixed solution of hydrochloric acid and ydrogen peroxide 50 (volume ratio 2: 5) boiled 0.5 hour in the mixed solution of ammoniacal liquor and ydrogen peroxide 50 (volume ratio 2: 5).With behind the deionized water repetitive scrubbing 100 ℃ of oven dry;
3. gained mica powder in the step 2 is mixed with the colloidal sol of gained in the 20ml step 1, stir, dry in fluidized-bed, obtain golden yellow powder after the grinding;
With resulting powder in the step 3 at 550 ℃ of following annealing reductase 12s hour, temperature rise rate is 10 ℃/min, feeds the 10ml/min argon gas in the annealing process, and in argon shield, cools off, and promptly obtains intelligent temperature-control functional mica vanadium nacreous pigment.
Embodiment 2
1. the 0.2g ammonium tungstate is dissolved in the 30ml deionized water, adds 4.0gV
2O
5Powder is made into suspension liquid, and stirring heating obtains the dry mixed powder behind the evaporate to dryness;
2. gained powder in the step 1 is heated 30 minutes down to fusing at 820 ℃, then melt is poured in the 300ml deionized water, stirred fast 2 hours, obtain dark-brown V after the filtration
2-xW
xO
5Colloidal sol was with still aging 48 hours of colloidal sol;
3. get the 5.0g white mica powder successively at absolute ethyl alcohol, the mixed solution of hydrochloric acid and ydrogen peroxide 50 (volume ratio 2: 5) boiled 0.5 hour in the mixed solution of ammoniacal liquor and ydrogen peroxide 50 (volume ratio 2: 5).With behind the deionized water repetitive scrubbing 100 ℃ of oven dry;
4. gained mica powder in the step 3 is mixed with the colloidal sol of gained in the 15ml step 2, the moisture evaporate to dryness of heated and stirred in system obtains golden yellow powder after the grinding;
With resulting powder in the step 4 at 550 ℃ of following annealing reductase 12s hour, temperature rise rate is 15 ℃/min, feeds 10ml/min nitrogen in the annealing process, and in nitrogen protection, cools off, and promptly obtains the intelligent temperature-control functional mica vanadium nacreous pigment after W mixes.
Embodiment 3
1. with 5.0gV
2O
5Powder is poured melt in the 600ml deionized water into 820 ℃ of heating extremely thawings in 30 minutes down then, stirs fast 2 hours, obtains dark-brown V after the filtration
2O
5Colloidal sol was with still aging 48 hours of colloidal sol;
2. get the 5.0g white mica powder successively at absolute ethyl alcohol, the mixed solution of hydrochloric acid and ydrogen peroxide 50 (volume ratio 2: 5) boiled 0.5 hour in the mixed solution of ammoniacal liquor and ydrogen peroxide 50 (volume ratio 2: 5).With behind the deionized water repetitive scrubbing 100 ℃ of oven dry;
3. gained mica powder in the step 2 is mixed with the colloidal sol of gained in the 20ml step 1, dry in fluidized-bed;
4. repeating step 3, improve sheet mica surface VO
2Film thickness obtains golden yellow powder after the grinding;
With resulting powder in the step 4 at 580 ℃ of following annealing reductase 12s hour, temperature rise rate is 20 ℃/min, feeds the 15ml/min argon gas in the annealing process, and in argon shield, cools off, and promptly obtains intelligent temperature-control functional mica vanadium nacreous pigment.
Embodiment 4
1. the 0.25g ammonium molybdate is dissolved in the 30ml deionized water, adds 4.0gV
2O
5Powder is made into suspension liquid, and stirring heating obtains the dry mixed powder behind the evaporate to dryness;
2. gained powder in the step 1 is heated 30 minutes down to fusing at 850 ℃, then melt is poured in the 400ml deionized water, stirred fast 2.5 hours, obtain dark-brown V after the filtration
2-xMo
xO
5Colloidal sol was with still aging 48 hours of colloidal sol;
3. get the 4.0g white mica powder successively at absolute ethyl alcohol, the mixed solution of hydrochloric acid and ydrogen peroxide 50 (volume ratio 2: 5) boiled 0.5 hour in the mixed solution of ammoniacal liquor and ydrogen peroxide 50 (volume ratio 2: 5).With behind the deionized water repetitive scrubbing 100 ℃ of oven dry;
4. gained mica powder in the step 3 is mixed with the colloidal sol of gained in the 15ml step 2, the moisture evaporate to dryness of heated and stirred in system obtains golden yellow powder after the grinding;
With resulting powder in the step 4 at 580 ℃ of following annealing reductase 12s hour, temperature rise rate is 15 ℃/min, feeds 10ml/min nitrogen in the annealing process, and in nitrogen protection, cools off, and promptly obtains the intelligent temperature-control functional mica vanadium nacreous pigment after Mo mixes.
1. the 0.15g Lanthanum trinitrate is dissolved in the 30ml deionized water, adds 4.0gV
2O
5Powder is made into suspension liquid, and stirring heating obtains the dry mixed powder behind the evaporate to dryness;
2. gained powder in the step 1 is heated 30 minutes down to fusing at 950 ℃, then melt is poured in the 400ml deionized water, stirred fast 2.5 hours, obtain dark-brown V after the filtration
2-xLa
xO
5Colloidal sol was with still aging 48 hours of colloidal sol;
3. get the 4.0g white mica powder successively at absolute ethyl alcohol, the mixed solution of hydrochloric acid and ydrogen peroxide 50 (volume ratio 2: 5) boiled 0.5 hour in the mixed solution of ammoniacal liquor and ydrogen peroxide 50 (volume ratio 2: 5).With behind the deionized water repetitive scrubbing 100 ℃ of oven dry;
4. gained mica powder in the step 3 is mixed with the colloidal sol of gained in the 15ml step 2, the moisture evaporate to dryness of heated and stirred in system obtains golden yellow powder after the grinding;
With resulting powder in the step 4 at 500 ℃ of following annealing reductase 12s hour, temperature rise rate is 15 ℃/min, feeds 10ml/min nitrogen in the annealing process, and in nitrogen protection, cools off, and promptly obtains the intelligent temperature-control functional mica vanadium nacreous pigment after La mixes.
Claims (6)
1. an intelligent temperature-control functional mica vanadium nacreous pigment is characterized in that, this pigment is made up of flaky mica powder and the sull that is coated on its surperficial one deck vanadium, and the general formula of this film is V
1-xM
xO
2, V is+4 valencys in the general formula, and M is W, Mo or La element, and x is between 0～0.25, and the optimization thickness of film is 30～300nm.
2. a kind of intelligent temperature-control functional mica vanadium nacreous pigment described in the claim 1 is characterized in that, surface coated general formula is V
1-xM
xO
2In the film, M is W, Mo or La element, can change the thermal induced phase transition temperature of mica vanadium nacreous pigment, and x is between 0～0.25 in the general formula.
3. method for preparing intelligent temperature-control functional mica vanadium nacreous pigment described in claim 1 is characterized in that step is following:
1) preparation V
2O
5Colloidal sol or contain the V of alloying element W, Mo or La
2O
5Colloidal sol;
2) the sheet mica micro mist is carried out surface treatment, remove its surface impurity ion, and the surface of etching sheet mica, reach certain wetting ability requirement;
3) on surface treated mica microplate, coat V
2O
5Colloidal sol, and make its drying become xerogel;
4) under certain temperature and atmosphere to the reduction of annealing of step 3 gained powder, obtain intelligent temperature-control functional mica vanadium nacreous pigment.
4. the method for claim 3, wherein V
2O
5The preparation method characteristic of colloidal sol does, with 2.0～5.0gV
2O
5Powder melts under at least greater than 550 ℃ high temperature, pours into rapidly in 300ml～600ml deionized water, and normal temperature stirred 2～5 hours down, obtained V after the filtration
2O
5The water-sol.
5. the method in claim 3 or the claim 4 is characterized in that, W, Mo or La element mix compound and the V that takes containing W, Mo or La element
2O
5The method of powder mixing congruent melting realizes.
6. the method for claim 3 is characterized in that, annealing reductive temperature is 400～650 ℃, and atmosphere is the mobile rare gas element, and flow velocity 5～60ml/min, annealing time are 0.5～6 hour.
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|---|---|---|---|
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|---|---|---|---|
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| CN103254664A (en) * | 2013-05-14 | 2013-08-21 | 四川大学 | Method for preparing intelligent temperature control type powder with mica coated by vanadium dioxide |
| CN109181650B (en) * | 2018-09-05 | 2020-12-04 | 长沙理工大学 | Dynamic thermal infrared stealth composite material based on double phase change and preparation method |
Citations (3)
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| WO2002010290A1 (en) * | 2000-07-27 | 2002-02-07 | Flex Products, Inc. | Composite reflective flake based pigments, method for their preparation and colorant comprising them |
| CN1621459A (en) * | 2004-10-28 | 2005-06-01 | 中山大学 | Intelligent vanadium dioxide solar temperature control coating |
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| WO2002010290A1 (en) * | 2000-07-27 | 2002-02-07 | Flex Products, Inc. | Composite reflective flake based pigments, method for their preparation and colorant comprising them |
| CN1791645A (en) * | 2003-05-21 | 2006-06-21 | 默克专利股份有限公司 | Photostabilised effect pigments |
| CN1621459A (en) * | 2004-10-28 | 2005-06-01 | 中山大学 | Intelligent vanadium dioxide solar temperature control coating |
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